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Metrohm Inline Sample Preparation
Intelligent injection techniques and automation solutions for complex sample preparation in ion chromatography analysis.

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28 Applications

AN-AUT-002
Automated sample handling and analysis with NOVA: Standard addition with the Metrohm 800 Dosino
The Metrohm 800 Dosino is the workhorse of any automated liquid handling setup. This instrument can be conveniently used in combination with the NOVA software and integrated conveniently with electrochemical measurements performed with the Autolab systems.
8.000.6037
Fully automated inline eluent preparation on demand
By using the 800 Dosino and the 849 Level Control as the only additional devices, Metrohm`s intelligent ion chromatography (IC) systems - the 850 Professional IC and the Compact IC family - can be easily extended to perform any unattended inline eluent preparation. Fully controlled by MagIC NetTM, the 849 Level Control monitors the eluent level while the Dosino performs all dosing and liquid handling tasks. Consecutive injections of a 250-µg/L standard over approximately 20 days revealed an excellent retention-time stability. After more than 800 consecutive injections, relative standard deviations for anions (F-, Cl-, NO2-, Br-, NO3-, PO43-, SO42-) and cations (Li+ , Na+, NH4+, K+, Ca2+, Mg2+) were smaller than 0.55 and 0.41%, respectively. In the case of a 24-hour sequence, retention-time precision for anions and cations was better than 0.09 and 0.08%, respectively. The presented inline eluent preparation system increases the retention-time reproducibility and allows the determination of anions and cations over a one-month period without manual eluent preparation.
8.000.6051
PC-controlled dosing and liquid handling
The 800 Dosino controlled by tiamo™ or Touch Control can be used universally for dosing and liquid handling tasks in both the analytical laboratory or directly in the synthesis laboratory. This poster looks at three typical liquid handling applications, the synthesis of metal-organic compounds, the preparation of standards, and the determination of pharmaceutical ingredients.
AN-C-096
Trace analysis of monovalent cations in an ethanolamine matrix (secondary cycle of a pressurized water reactor) using Metrohm Inline Sample Preparation with an 800 Dosino for liquid handling
Methylamine (MMA), dimethylamine (DMA), and trimethylamine (TMA) in methylpyrrolidone using Metrohm Inline Matrix Elimination.
AN-S-315
Methanedisulfonic acid in chromium baths using nested dilution, Dosino Regeneration and STREAM
Methanedisulfonic acid (MDSA) is used as a catalyst in chromium plating baths. The MDSA concentration in the bath must be known in order to monitor the chromating. The analysis of a bath sample requires dilution by a factor of 2,500. This Application Note shows the automatic Inline Dilution that takes place in two steps. While one sample is being analyzed, the time-optimized dilution of the next sample is already running. The MSM is regenerated using an 800 Dosino and the STREAM setup: The eluent is used for rinsing the regenerated MSM after exiting the detector.
8.000.6089
Automated sample measurement in Karl Fischer titration
This poster describes a method for automated and precise dosing of liquid samples into the Karl Fischer titration cell using Metrohm Dosino liquid handling technology. First, the titer was automatically determined with ultrapure water. The same dosing procedure proved valuable for the automated water determination in highly viscous water-glycol fluids and low-boiling organic solvents such as n-pentane. Lastly, the method copes with the labor-intensive and human error-prone suitability test stipulated in chapter 2.5.12 in the European Pharmacopoeia.
8.000.6055
Liquid handling applied to automated sample preparation in liquid chromatography
In routine chemical analysis, the predominant challenge involves a higher sample throughput, improved reproducibility, liquid handling flexibility and reduced personnel costs. In response to these requirements, the 872 Extension Module Liquid Handling in combination with the MagIC NetTM software and the well-proven Dosino technology expands the possibilities of inline sample preparation and opens up new fields of application. Among others, the module can be used, together with an optional mixing vessel, for pH adjustments, pre-column derivatizations, or the mixing of solutions.As a representative of an inline sample preparation technique, this poster describes the performance of precise dilutions. By using only one single stable standard solution, multi-point calibration curves can be automatically recorded by diluting a concentrated standard in an external vessel.
8.000.6012
Automated logical dilution for ion chromatographic determinations
The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of sophisticated ion chromatographic sample preparation techniques. One of these is the automated inline dilution of samples.After the first sample injection, MagIC NetTM verifies if the area of the sample peak lies within the calibration range. If the measured peak area is outside these limits, the software calculates the appropriate dilution factor, dilutes and automatically re-injects the sample. For all investigated ions (Li+, Na+, K+, Ca2+, Mg2+, F-, Cl- , NO2-, Br-, NO3-, SO42- ), automated logical dilution yielded coefficients of determination (R2) better than 0.9999. Direct-injection recoveries for cations and anions were within 98.6…99.5% and 93.4…100.4% respectively. In contrast, after logical dilution, recoveries for cations and anions were within 100.1…102.9% and 98.2…102.6% respectively. The relative standard deviations for all determinations involving diluted sample solutions were smaller than 0.91%.
8.000.6042
Straightforward multipoint calibration using a single standard
The combination of 850 Professional IC, 858 Professional Sample Processor, Dosino and MagIC NetTM software offers a variety of automated ion chromatographic sample preparation and calibration techniques available as an anion, cation or dual channel system. Calibration is straightforward and requires only one multi-ion standard.Inline calibration allows the calibration of any standard concentration in the ppt range by using one single stable standard solution at the ppb level. By using a preconcentration column and switching the valves one, two or more times different calibration concentrations at the ultra-trace level can be created with unprecedented reproducibility. The inline preconcentration technique uses a pre-concentration column and is ideally suited for trace analysis in complex matrices, especially when combined with matrix elimination. Besides facilitating the preparation of g/L to ng/L calibration graphs Metrohm`s intelligent techniques are capable of logical decision making. While Metrohm`s intelligent Partial Loop technique (MiPT) allows samples with a wide concentration range to be injected without previous manual dilution, the intelligent inline dilution technique, after the first sample injection, compares peak areas, calculates, if necessary, the dilution factor, dilutes and automatically re-injects the sample. The presented inline techniques allow the rationalization of the time-consuming, error-prone and cost-intensive manual preparation of standard solutions. They guarantee that the determined sample concentrations always lie within the calibration range. Higher sample throughputs as well as lower analysis costs and improved data reliability are achieved.
AN-P-047
Determination of sugars and sugar alcohols using pulsed amperometric detection and Dose-in Gradient
The determination of sugar and sugar alcohols is very important for food analysis. The Dose-in Gradient system extends the gradient capability of the standard IC system. The isocratic system is expanded to form a binary gradient system with just one 800 Dosino and one T-piece.
AN-S-304
Variable Inline Preconcentration including Matrix Elimination for trace anion analysis (MiPCT-ME)
Metrohm Inline Preconcentration Technique with Matrix Elimination (MiPCT-ME) is a powerful tool that combines preconcentration, matrix elimination, and multilevel calibration. The latter only requires a single multi-ion standard solution. The 800 Dosino takes over all liquid handling tasks. The shown system setup allows sample analysis from 0.1 µg/L up to 1.0 mg/L.
AN-C-134
Cation Inline Eluent Preparation using an 849 Level Control.
Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the required eluent concentration. The use of eluent concentrates is suitable for any eluent. This facilitates unattended operation of the system over several weeks (see AN S-296 for anion eluent preparation).
AN-C-148
Metrohm Inline Dilution – Dilution factors of up to 10,000 in two intelligent steps
Sample dilution is a work-intensive routine task in the analysis laboratory. An automatic two-step dilution exponentiates the dilution factor – 1:100 – thus incorporating a dilution factor of 10,000. The intelligent dilution is made possible by MagIC Net, which calculates the essential dilution steps, and by the dosing properties of the 800 Dosino and the Liquid Handling Station. The Application Note shows statistical results of a 1:10,000 dilution.
AN-S-305
Determination of chlorate, thiosulfate, thiocyanate, and perchlorate in the presence of standard anions using a Dose-in Gradient
The Dose-in Gradient expands the standard IC system to a gradient system. Using isocratic elution for separating the oxyhalides and the anions containing sulfur is very time-consuming. An 800 Dosino and a T-piece are used to expand the isocratic system to a binary gradient system. This is shown in the example of the determination of the standard anions, in addition to chlorate, thiosulfate, thiocyanate, and perchlorate.
AN-S-296
Anion Inline Eluent Preparation using an 849 Level Control
Eluent preparation on demand (EPOD) is the convenient and flexible way of automatic eluent preparation. The 849 Level Control together with an 800 Dosino equipped with a 50 mL dosing unit are used to dilute an eluent concentrate to the final eluent concentration. The use of eluent concentrates is suitable for any type of eluent. This facilitates unattended operation of the system over several weeks (see AN C-134 for cation eluent preparation).
AN-U-058
Chromate in dye samples using post-column reaction and subsequent UV/VIS detection
Dye samples are analyzed for trace chromate. Chromate (Cr(VI)) is considered toxic and potentially carcinogenic for which reason its concentrations should be as low as possible. This sample is prepared with C18 cartridges and injected applying Metrohm intelligent Preconcentration Technique (MiPCT). After each injection, the preconcentration column requires additional rinsing to eliminate matrix effects. For this purpose, no other instrument than an 800 Dosino is required. The system is optimized for sample volumes between 20 and 2000 µL. For most samples additional rinsing of the preconcentration column is not required.
AB-420
Determination of suppressor with CVS using the calibration technique «smartDT» with dynamic addition volumes
The Application Bulletin describes the determination of suppressor in acid copper baths by smartDT. The determination of suppressor with dilution titration (DT) involves numerous additions with standard solution or sample to reach the evaluation ratio. Usually fixed, equidistant addition volumes are used. With smartDT, variable addition volumes are used that are dynamically calculated by the software. At the beginning, the volumes are bigger. Towards the evaluation ratio, the addition volume becomes smaller to guarantee a good accuracy of the result. The operator defines the first and the smallest addition volume to be used. All volumes in between are calculated by the software considering the progress of the determination. The time saving with smartDT compared to a classic DT with fixed addition volumes can be up to 40%. smartDT is suitable for nonlinear regression and quadratic regression as well as linear interpolation. It can be used for determination of suppressor in acid copper baths as well as in tin and tin-lead baths and works with 1, 2, and 3 mm Pt working electrodes. A 800 Dosino is required for the automatic addition of suppressor standard or sample. The method can also be used in fully automated systems.
AN-T-223
Analysis of electroplating baths
Electroplating processes are used in several different industry sectors to protect the surface quality of various products against corrosion or abrasion and significantly improve their working life. It is essential to check the bath composition on a regular basis to ensure that the process is operating correctly. Typical examples of electroplating baths include alkaline degreasing baths or acidic or alkaline baths containing metals e.g. copper, nickel, or chromium, or components like chloride and cyanide. It is crucial that the chosen analysis technique fulfills high safety standards for these kinds of analyses and produces reliable results. The OMNIS Sample Robot system automatically pipettes and analyzes aggressive electroplating bath samples on different workstations, increasing the safety in the lab. This provides more reliable results in comparison to manual titration and is more time efficient as different parameters can be analyzed in parallel.
AN-S-403
Anions in lithium-ion battery solvents
N-Methylpyrrolidone (NMP) is crucial for lithium-ion battery production. Metrohm’s intelligent Preconcentration Technique with Matrix Elimination enables µg/L-level anion analysis in NMP.
AN-S-379
Fluoride in sodium fluoride tablets for pharmaceutical use
Sodium fluoride tablets for pharmaceutical use need to comply with U.S. Pharmacopeia (USP) requirements. Ion chromatography (IC) with suppressed conductivity detection has been approved by the USP as a validated method to quantify fluoride content in sodium fluoride tablets. In the course of the USP monograph modernization, using automated IC makes this type of analysis even easier.
AN-S-380
Monofluorophosphate and fluoride in sodium monofluorophosphate for pharmaceutical use
Ion chromatography (IC) with suppressed conductivity detection has been approved by the U.S. Pharmacopeia (USP) as a validated method to quantify the monofluorophosphate (MFP) content in sodium monofluorophosphate. This Application Note shows that all acceptance criteria for the USP Monograph «Sodium Monofluorophosphate» are fulfilled and the procedure was approved as a validated USP method.
AN-S-372
Analysis of Li-ion battery electrolytes with ion chromatography
Lithium-ion (Li-ion) battery electrolyte quality is essential for performance, stability, and safety reasons. Ion chromatography is an accurate method for electrolyte analysis.
AN-NIR-071
Automated acid number determination in lubricants with near-infrared spectroscopy
Acid Number (AN) analysis of lubricants (ASTM D664) can be a lengthy and costly process due to usage of large amounts of chemicals and required cleaning steps of the analytical equipment between each measurement. This application note demonstrates that the XDS RapidLiquid Analyzer operating in the visible and near-infrared spectral region (Vis-NIR) provides a cost-efficient, fast alternative for the determination of the acid number of lubricants. With no sample preparation or chemicals needed, Vis-NIR spectroscopy allows for the analysis of AN in less than a minute.
AN-U-076
Zinc Oxide Assay as per USP General Chapter <591>
Manufacturers and laboratories must use validated methods to determine the zinc content in skin care products and pharmaceutical supplements to meet strict quality standards set by the United States Pharmacopeia and National Formulary (USP-NF). USP-NF has updated the zinc monograph (General Chapter <591>, Zinc Determination) and replaced the existing identification procedure of titration with ion chromatography (IC). The analysis involves separating Zn using a Metrosep A Supp 10 column followed by post-column reaction using 4-(2-pyridylazo)resorcinol and detection at 530 nm.
AN-S-376
Fluoride in sodium fluoride gel for pharmaceutical use
Sodium fluoride gel for pharmaceutical use needs to comply with USP requirements. The actual monograph (USP 42) uses two different methods for the identification and the assay. Ion chromatography allows the analysis of these two parameters in one single determination. In the course of the USP monograph modernization, this ion chromatographic approach makes this type of analysis even easier.
AN-RS-048
Phosphates speciation with Raman spectroscopy
Metrohm’s MIRA XTR handheld Raman spectrometer enables fast, reagent-free identification of phosphate species, enabling continuous monitoring of dynamic systems.
AN-S-375
Fluoride in sodium fluoride for pharmaceutical use
Dental care products often contain sodium fluoride as an active ingredient. Manufacturers use the United States Pharmacopeia and National Formulary (USP-NF) Monograph «Sodium Fluoride» to quantify sodium fluoride and its anionic contaminants chloride and acetate in these products. The validated USP method proposes ion chromatography (IC) with suppressed conductivity detection to carry out the fluoride assay as well as the impurity determination in a single chromatogram.
AN-CIC-033
Monitoring PFASs in water sources
AOF (adsorbable organic fluorine) is used to screen for per- and polyfluorinated alkyl substances in aqueous matrices via pyrohydrolytic combustion and ion chromatography.

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Ion chromatographs
Ion chromatography instruments for routine use and research applications: flexible, reliable, and easy to use.

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